反应 #2111273
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07754732B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2-Isopropyl-6-methyl-phenylamine (5 g, 33.5 mmol) was dissolved in acetic acid (20 mL). To this solution was added a solution of bromine (1.8 mL, 35.14 mmol) in acetic acid (5 mL) dropwise over 10 min. After stirring for 1 h at room temperature, the reaction mixture was diluted with methylene chloride, washed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), and brine. The organic phase was dried over sodium sulfate, filtered, and concentrated. Purification by flash chromatography on silica gel afforded 7.6 g (quantitative) of the desired product. LC/MS: tR=1.37 min, 230.07 (MH)+. washed with water (2×), saturated sodium thiosulfate (2×), saturated sodium bicarbonate (2×), and brine The organic phase was dried over sodium sulfate filtered concentrated Purification by flash chromatography on silica gel
来源 ID: ord-53054fc6f2674f7a966d77ff97c47160